A kind of preparation method of lorcaserin intermediate
A technology for lorcaserin and intermediates, applied in the field of preparation of lorcaserin intermediates, can solve the problems of high price, high toxicity of HBr, increase production cost and the like, achieve easy storage and use, avoid industrial waste water, save energy The effect of production costs
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Embodiment 1
[0040] Embodiment 1: the synthesis of p-chlorophenethylamine
[0041]
[0042] Add 50.0g of p-chlorophenylacetonitrile, 22.0g of sodium borohydride and 500ml of tetrahydrofuran into a 1000ml four-neck flask, stir under nitrogen protection, and cool down in an ice-salt bath. When the system temperature is 0~5°C, add 88.4g of boron trifluoride ether Add it into a 1000mL four-necked bottle through a constant pressure dropping funnel. During the dropping process, control the temperature of the reaction system at 0-10°C. A large amount of gas will be generated during the dropping process. After the dropping is completed, a large amount of white solid will be generated in the reaction system. Heat up to 25~35°C and stir for 1 hour, then raise the temperature to 45~55°C and stir for 4~6 hours, follow the reaction by HPLC until the content of p-chlorophenylacetonitrile in the raw material is less than 1.0%, stop heating, cool down to 0~5°C, pass constant pressure Add 20ml of water ...
Embodiment 2
[0043] Embodiment 2: the synthesis of p-chlorophenethylamine
[0044]
[0045] Add 50.0g of p-chlorophenylacetonitrile, 20.0g of sodium borohydride and 500ml of 2-methyltetrahydrofuran into a 1000ml four-necked flask, stir under nitrogen protection, and cool down in an ice-salt bath. When the system temperature is 0~5°C, add 75.0g of Boron fluoride ether was added into a 1000ml four-necked bottle through a constant pressure dropping funnel. During the dropping process, the temperature of the reaction system was controlled at 0-10°C. A large amount of gas was generated during the dropping process. After the dropping, the reaction system had a large amount of gas. A white solid is formed, heat up to 25~35°C and stir for 1 hour, then heat up to 45~55°C and stir for 4~6 hours, follow the reaction by HPLC until the content of p-chlorophenylacetonitrile in the raw material is less than 1.0%, stop heating, and cool down to 0~5°C , add 20ml of water dropwise through the constant pr...
Embodiment 3
[0046] Embodiment 3: Synthesis of lorcaserin intermediate I
[0047]
[0048] Add 30.0g of 1-chloro-2-propanol, 88.0g of potassium carbonate and 500ml of acetonitrile into a 1000ml four-neck flask, stir under nitrogen protection, control the temperature of the system at 20~25°C, and constant Add the pressure drop funnel into a 1000ml four-necked bottle, control the dropping speed, and control it at 30.0~40.0min. After the dropwise addition is completed, raise the temperature to 55~60°C and stir for 8~10 hours, and follow the reaction by HPLC until the content of p-chlorophenethylamine in the raw material is reached. Less than 1.0%, remove acetonitrile by distillation under reduced pressure, add 300ml water and 500ml ethyl acetate to extract, separate layers, remove ethyl acetate by distillation under reduced pressure to obtain a light yellow solid, and the solid is recrystallized with ethyl acetate and n-heptane (ethyl acetate The volume ratio of n-heptane and n-heptane is ...
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